CN107254285A - A kind of preparation method of the water-fast jelly of hardware bonding - Google Patents
A kind of preparation method of the water-fast jelly of hardware bonding Download PDFInfo
- Publication number
- CN107254285A CN107254285A CN201610995164.1A CN201610995164A CN107254285A CN 107254285 A CN107254285 A CN 107254285A CN 201610995164 A CN201610995164 A CN 201610995164A CN 107254285 A CN107254285 A CN 107254285A
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- epoxy resin
- bisphenol
- curing agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1494—Polycondensates modified by chemical after-treatment followed by a further chemical treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of preparation method of the water-fast jelly of hardware bonding, concretely comprise the following steps:1)Preparation prepares the raw material of bisphenol-A epoxy resin first, then prepares bisphenol-A epoxy resin stand-by;2)Then the modification operation of bisphenol-A epoxy resin is carried out, addition modifying agent and the bisphenol-A epoxy resin prepared carry out heating response, and obtain modified epoxy;3)Then mixed curing agent is prepared, the mixed curing agent includes 25 58 parts of diaminodiphenyl-methane curing agent, 6 15 parts of expoxy propane o-cresyl ether, 13 25 parts of filler, 9 17 parts of EP rubbers, 6 12 parts of DOPO fire retardants;4)After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.The present invention method by rationally controlling each reactant between proportioning, rationally control reaction condition and prepare a kind of High-durability epoxy resin adhesive.
Description
Technical field
The present invention relates to high-molecular gel field, a kind of preparation side of the water-fast jelly of hardware bonding is specifically referred to
Method.
Background technology
The adhesive product that hardware adhesive is commonly used as building trade is widely used in construction and house
Portion is fitted up, and for house inside fitting, hardware adhesive can be usually used in metallic article.And conventional at present
Hardware adhesive usually contains the organic poisons such as aldehydes, and its release can influence health.So, how to solve metal structure
Part discharges the technical problem that dusty gas is urgent need to resolve with glue.
And epoxyn as a kind of environment-friendly type gel rubber material the problem of can solve the problem that existing building adhesive, institute
The epoxyn stated is the work that a class is formulated by epoxy resin base-material, curing agent, diluent, accelerator and filler
Journey adhesive.Because its adhesive property is good, feature is good, less expensive, technique for sticking easy, so existing in recent decades
Household electrical appliances, automobile, water conservancy traffic, electronic apparatus and aerospace industry field are widely used.With new and high technology and nanometer
Technology is continued to develop, and in recent years, the modification to epoxy resin deepens continuously, and interpenetrating networks, chemical copolymerization and nano-particle increase
The method extensive use such as tough, by epoxy preparation into various high-performance adhesive kinds it is also more and more.But it has one
Individual obvious shortcoming is toughness deficiency, easily poor impact resistance, cracking after solidification, and the shortcoming greatly limit answering for epoxy resin
With.The characteristic requirements more and more highers developed rapidly to epoxy resin of various materials, epoxy resin is solidified into epoxy resin
The emphasis of use research, people carry out solidification toughness reinforcing using a variety of methods to epoxy resin, so that its application field is more
Extensively.
The content of the invention
It is an object of the invention to provide a kind of being used in hardware bonding and with efficient moistureproof water-fast function
The preparation method of adhesive.
The present invention is achieved through the following technical solutions:A kind of preparation method of the water-fast jelly of hardware bonding, tool
Body step is:
(1)Preparation prepares the raw material of bisphenol-A epoxy resin first, then prepares bisphenol-A epoxy resin
It is stand-by;
(2)Then the modification operation of bisphenol-A epoxy resin, addition modifying agent and the hydrogenated bisphenol A type prepared are carried out
Epoxy resin carries out heating response, and obtains modified epoxy;
(3)Then mixed curing agent is prepared, the mixed curing agent includes 25-58 parts of diaminodiphenyl-methane curing agent, ring
6-15 parts of Ethylene Oxide o-cresyl ether, 13-25 parts of filler, 9-17 parts of EP rubbers, 6-12 parts of DOPO fire retardants;
(4)After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.
Further, the step(1)It is middle to prepare concretely comprising the following steps for bisphenol-A epoxy resin:
(1.1)Prepare raw material, the raw material is sodium hydroxide, epoxychloropropane, hydrogenated bisphenol A and methyl iso-butyl ketone (MIBK);
(1.2)Represented with parts by weight, take 3-4 parts of sodium hydroxide, 19-31 parts of epoxychloropropane, 9-13 parts of A Hydrogenated Bisphenol A
A, methyl iso-butyl ketone (MIBK) is simultaneously added in reactor by a certain percentage, and adds catalyst, then 50-60 DEG C of water bath with thermostatic control and is stirred
Mix;Then condensing reflux reacts 24h;
(1.3)Then add after deionized water is sufficiently mixed and staticly settle after question response terminates, after then upper aqueous layer is filtered out
Surplus solution is heated to 75 DEG C and sodium hydroxide solution is added, then constant temperature stirring reaction 2.5-3.5h;
(1.4)Distilled water washing point liquid is added after question response, until when the water layer pH value separated is neutral, filtrate is completely distilled off
Later, light yellow, transparent bisphenol-A epoxy resin is obtained.
Further, the step(1.3)In sodium hydroxide mass fraction be 19-31%, the step(1.4)In
Vapo(u)rizing temperature be 95-96 DEG C.
Further, the step(2)In modification operation concretely comprise the following steps:
(2.1)Modifying agent is got out, the modifying agent is vinyl acetate latex and dibutyl phthalate latex, by two kinds
Dry for standby after latex demulsification;
(2.2)Then vinyl acetate latex is added in bisphenol-A epoxy resin, then for 120-140 DEG C of temperature
Under the conditions of react 2-4h;
(2.3)Question response adds dibutyl phthalate latex after terminating, 1- is reacted under 120-140 DEG C of temperature conditionss
1.2h, that is, obtain the modified epoxy for thick liquid under normal temperature.
Further, the step(3)In prepare concretely comprising the following steps for mixed curing agent:
(3.1)Get out mix the raw material of fixative, the raw material are represented with parts by weight, including diaminodiphenyl-methane
25-58 parts of curing agent, 6-15 parts of expoxy propane o-cresyl ether, 13-25 parts of filler, 9-17 parts of EP rubbers, DOPO fire retardants
6-12 parts;
(3.2)The filler first taken diaminodiphenyl-methane curing agent and add EP rubbers sum thereto carries out Hybrid Heating
1-2h is stirred, it is slow in whipping process to add expoxy propane o-cresyl ether thereto;
(3.3)Then DOPO fire retardants are added and continue constant temperature stirring 30-50min, mixing fixative is produced.
Heretofore described bisphenol-A epoxy resin chemical name be hydrogenated bisphenol A diglycidyl ether, be by
The hexahydro bisphenol-A that bisphenol-A hydrogenation is obtained is obtained with epoxychloropropane in sodium hydroxide catalyzed lower polycondensation.Be a kind of viscosity very
The fairly good epoxy resin of low, gel time length, weatherability.Further, the filler is aluminum oxide.
The present invention compared with prior art, with advantages below and beneficial effect:
The method of the present invention by rationally controlling each reactant between proportioning, rationally control reaction condition and prepare a kind of height
Solidify obtained from endurance quality epoxy resin adhesive, the epoxy resin composition that epoxy resin of the invention is obtained
Thing, with the mechanical properties such as moisture-proof, excellent heat resistance, and impact resistance also excellent performance, adhesive property is good, durability
Can be good, and preparation method is simple and easy to apply, is adapted to industrialized production, is compared compared with other epoxy resin adhesives, is bonded without strict
The metal of surface treatment and it is nonmetallic all have good adhesive property and endurance quality, can be applied to adhesive field.
Embodiment
Embodiments of the invention are described below in detail.
Embodiment 1:
A kind of water-fast jelly of hardware bonding of the present embodiment, is represented with parts by weight, including hydrogenated bisphenol A type asphalt mixtures modified by epoxy resin
80-210 parts of aliphatic radical material, 25-58 parts of diaminodiphenyl-methane curing agent, 6-15 parts of expoxy propane o-cresyl ether, filler 13-
25 parts, 9-17 parts of EP rubbers, 6-12 parts of DOPO fire retardants.
The preparation method of the present invention, is concretely comprised the following steps:
(1)Preparation prepares the raw material of bisphenol-A epoxy resin first, is represented with parts by weight, takes 3-4 parts of hydroxide
Sodium, 19-31 parts of epoxychloropropane, 9-13 parts of hydrogenated bisphenol A, methyl iso-butyl ketone (MIBK) simultaneously adds reactor by a certain percentage
In, and catalyst is added, then 50-60 DEG C of water bath with thermostatic control and stirred;Then condensing reflux reacts 24h;
(2)Then add after deionized water is sufficiently mixed and staticly settle after question response terminates, will after then upper aqueous layer is filtered out
Surplus solution is heated to 75 DEG C and adds sodium hydroxide solution, then constant temperature stirring reaction 1-3h;Distilled water is added after question response
Washing point liquid, until when the water layer pH value separated is neutrality, after filtrate is completely distilled off, obtaining light yellow, transparent hydrogenation
Bisphenol A type epoxy resin;
(4)Then the modification operation of bisphenol-A epoxy resin is carried out, modifying agent is got out, the modifying agent is acetic acid second
Alkene ester latex and dibutyl phthalate latex, by dry for standby after two kinds of latex demulsifications;Then by vinyl acetate latex
Add in bisphenol-A epoxy resin, then react 2-4h under for 120-140 DEG C of temperature conditionss;Question response terminate after again
Dibutyl phthalate latex is added, 1-1.2h is reacted under 120-140 DEG C of temperature conditionss, that is, it is thick shape liquid under normal temperature to obtain
The modified epoxy of body;
(5)Then mixed curing agent is prepared by raw material of diaminodiphenyl-methane curing agent, 25-58 parts of diaminourea is first taken
Diphenyl methane curing agent, and 9-17 parts of EP rubbers and 13-25 parts of filler progress Hybrid Heating stirring 1-2h are added,
The slow expoxy propane o-cresyl ether for adding 6-15 parts thereto in whipping process;Then the DOPO for adding 6-12 parts is fire-retardant
Agent continues constant temperature stirring 30-50min, produces mixing fixative;
(6)After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.
Embodiment 2:
A kind of water-fast jelly of hardware bonding of the present embodiment, is represented with parts by weight, the hydrogenated bisphenol A type asphalt mixtures modified by epoxy resin
150 parts of aliphatic radical material, 40 parts of diaminodiphenyl-methane curing agent, 6 parts of expoxy propane o-cresyl ether, 10 parts of filler, the rubber of second third
8 parts of glue, 9 parts of DOPO fire retardants.
Embodiment 3:
A kind of water-fast jelly of hardware bonding of the present embodiment, is represented with parts by weight, the hydrogenated bisphenol A type asphalt mixtures modified by epoxy resin
200 parts of aliphatic radical material, 48 parts of diaminodiphenyl-methane curing agent, 7 parts of expoxy propane o-cresyl ether, 14 parts of filler, the rubber of second third
12 parts of glue, 12 parts of DOPO fire retardants.
Embodiment 4:
A kind of water-fast jelly of hardware bonding of the present embodiment, is represented with parts by weight, the hydrogenated bisphenol A type asphalt mixtures modified by epoxy resin
250 parts of aliphatic radical material, 55 parts of diaminodiphenyl-methane curing agent, 9 parts of expoxy propane o-cresyl ether, 20 parts of filler, the rubber of second third
17 parts of glue, 15 parts of DOPO fire retardants.
Then the water-resistant adhesive of three kinds of different formulations ratios of embodiment 2 ~ 4 is subjected to detection contrast, to verify this hair
Bright implementation result.
1st, adhesive strength is tested:Take one group(4)The ligneous piece of same specification, in each ligneous piece, corresponding contact surface is pressed
Every square metre of glue coating of 100g, the specification of each contact surface is 80mm × 40mm, afterwards by the contact surface pair of Liang Ge ligneous pieces
Compression should be overlapped, closed assembly time is no more than 20 minutes, and contact surface applies 0.85-1.20Mpa pressure, and at room temperature, installation time 8 is small
When, place 16 hours after pressure relief, make a strength test again;4 repetitions, average;
2nd, bending strength is tested:Take one group(4)The plastic part of same specification, the modeling referring next to state marked as GB1042-79
Material bend test method is tested, and the specification of every group of plastic part is 100 × 20 × 15mm;
3rd, compressive strength is tested:Take one group(4)The plastic part of same specification, the modeling referring next to state marked as GB1041-79
Material compression test method is tested, and the cross-sectional dimensions for the plastic part tested are 20 × 15mm, a height of 10mm;
4th, water resistance test:Take one group(4)The ligneous piece of same specification, it is every by 100g in the corresponding contact surface of each ligneous piece
Square metre cementing, the specification of each contact surface is 80mm × 40mm, and the contact surface correspondence of Liang Ge ligneous pieces is overlapped into pressure afterwards
Tightly, spontaneously dry 8 hours, soaked in 32-40 DEG C of water, measure is come unglued the time, and 4 repetitions are averaged;
5th, hardening time tests:Take bisphenol-A epoxy resin 5g to be placed in beaker, keep bar of the room temperature at 20-25 DEG C
Under part, take mixed curing agent 2.0-2.5g to add in beaker, and stir standing after 15-20min and test its hardening time, 4 weights
Average again.
Table 1
Will according to the adhesive strength of the results showed that embodiment of the present invention 2 ~ 4, bending strength, compressive strength and water resistance
It is better than the comparative example using ordinary epoxy resin adhesive, and hardening time will also be less than ordinary epoxy resin adhesive,
And between three embodiments of the present invention, it can be seen that all test indexs all show the formula rate of the present invention in certain limit
It is interior to reach preferable effect, obvious difference occurs if too small or too big, and pass through to institute by the present invention
There is the collaboration between the adjustment of component proportion, each component, both keep high intensity, there can be preferable water resistance again, with aobvious
The novelty of work.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that:Not
A variety of change, modification, replacement and modification can be carried out to these embodiments by departing under the principle and objective of the present invention, of the invention
Scope is limited by claim and its equivalent.
Claims (5)
1. a kind of preparation method of the water-fast jelly of hardware bonding, it is characterized in that being:Concretely comprise the following steps:
(1)Preparation prepares the raw material of bisphenol-A epoxy resin first, then prepares bisphenol-A epoxy resin
It is stand-by;
(2)Then the modification operation of bisphenol-A epoxy resin, addition modifying agent and the hydrogenated bisphenol A type prepared are carried out
Epoxy resin carries out heating response, and obtains modified epoxy;
(3)Then mixed curing agent is prepared, the mixed curing agent includes 25-58 parts of diaminodiphenyl-methane curing agent, ring
6-15 parts of Ethylene Oxide o-cresyl ether, 13-25 parts of filler, 9-17 parts of EP rubbers, 6-12 parts of DOPO fire retardants;
(4)After modified epoxy and mixed curing agent are independently encapsulated, then packed products together two-by-two.
2. a kind of preparation method of the water-fast jelly of hardware bonding according to claim 1, it is characterised in that:Institute
State step(1)It is middle to prepare concretely comprising the following steps for bisphenol-A epoxy resin:
(1.1)Prepare raw material, the raw material is sodium hydroxide, epoxychloropropane, hydrogenated bisphenol A and methyl iso-butyl ketone (MIBK);
(1.2)Represented with parts by weight, take 3-4 parts of sodium hydroxide, 19-31 parts of epoxychloropropane, 9-13 parts of A Hydrogenated Bisphenol A
A, methyl iso-butyl ketone (MIBK) is simultaneously added in reactor by a certain percentage, and adds catalyst, then 50-60 DEG C of water bath with thermostatic control and is stirred
Mix;Then condensing reflux reacts 24h;
(1.3)Then add after deionized water is sufficiently mixed and staticly settle after question response terminates, after then upper aqueous layer is filtered out
Surplus solution is heated to 75 DEG C and sodium hydroxide solution is added, then constant temperature stirring reaction 2.5-3.5h;
(1.4)Distilled water washing point liquid is added after question response, until when the water layer pH value separated is neutral, filtrate is completely distilled off
Later, light yellow, transparent bisphenol-A epoxy resin is obtained.
3. a kind of preparation method of the water-fast jelly of hardware bonding according to claim 2, it is characterised in that:Institute
State step(1.3)In sodium hydroxide mass fraction be 19-31%, the step(1.4)In vapo(u)rizing temperature be 95-96 DEG C.
4. a kind of preparation method of the water-fast jelly of hardware bonding according to any one of claim 1 ~ 3, it is special
Levy and be:The step(2)In modification operation concretely comprise the following steps:
(2.1)Modifying agent is got out, the modifying agent is vinyl acetate latex and dibutyl phthalate latex, by two kinds
Dry for standby after latex demulsification;
(2.2)Then vinyl acetate latex is added in bisphenol-A epoxy resin, then for 120-140 DEG C of temperature
Under the conditions of react 2-4h;
(2.3)Question response adds dibutyl phthalate latex after terminating, 1- is reacted under 120-140 DEG C of temperature conditionss
1.2h, that is, obtain the modified epoxy for thick liquid under normal temperature.
5. a kind of preparation method of the water-fast jelly of hardware bonding according to any one of claim 1 ~ 3, it is special
Levy and be:The step(3)In prepare concretely comprising the following steps for mixed curing agent:
(3.1)Get out mix the raw material of fixative, the raw material are represented with parts by weight, including diaminodiphenyl-methane
25-58 parts of curing agent, 6-15 parts of expoxy propane o-cresyl ether, 13-25 parts of filler, 9-17 parts of EP rubbers, DOPO fire retardants
6-12 parts;
(3.2)The filler first taken diaminodiphenyl-methane curing agent and add EP rubbers sum thereto carries out Hybrid Heating
1-2h is stirred, it is slow in whipping process to add expoxy propane o-cresyl ether thereto;
(3.3)Then DOPO fire retardants are added and continue constant temperature stirring 30-50min, mixing fixative is produced.
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CN201610995164.1A CN107254285A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of the water-fast jelly of hardware bonding |
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CN201610995164.1A CN107254285A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of the water-fast jelly of hardware bonding |
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Citations (1)
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CN105062395A (en) * | 2015-08-21 | 2015-11-18 | 广州市白云化工实业有限公司 | Two-component epoxy glue and preparation method thereof |
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CN105062395A (en) * | 2015-08-21 | 2015-11-18 | 广州市白云化工实业有限公司 | Two-component epoxy glue and preparation method thereof |
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Application publication date: 20171017 |